CN108693241A - Method that is a kind of while measuring selenium and cadmium in soil - Google Patents
Method that is a kind of while measuring selenium and cadmium in soil Download PDFInfo
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- CN108693241A CN108693241A CN201810296494.0A CN201810296494A CN108693241A CN 108693241 A CN108693241 A CN 108693241A CN 201810296494 A CN201810296494 A CN 201810296494A CN 108693241 A CN108693241 A CN 108693241A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
It the invention belongs to environmental analysis detection technique field, discloses a kind of using Dynamic Reaction Cell-inductively coupled plasma mass spectrometry while the method that measures selenium and cadmium in soil, specifically includes:(1) resolution processing is carried out to sample to be tested;(2) solution after Dynamic Reaction Cell-inductively coupled plasma mass spectrometry detection resolution is used.The present invention handles sample to be tested by resolution, selenium in soil and cadmium are measured simultaneously using Dynamic Reaction Cell-inductively coupled plasma mass spectrometry, by the reaction gas flow velocity and RPq values that optimize Dynamic Reaction Cell, it effectively reduces interference and improves detection limit, improve the accuracy and sensitivity of detection.
Description
Technical field
The invention belongs to environmental analysis detection technique field, it is related to selenium and Cadmium detrmination method in a kind of soil, more specifically
Ground is related to a kind of using Dynamic Reaction Cell-inductively coupled plasma mass spectrometry while the method that measures selenium and cadmium in soil.
Background technology
Selenium (Se) is the essential trace element of human life health, has the function of multi-biological, if intake is not
Foot, or consume are excessive, will cause a variety of diseases, selenium also has effects that anticancer in addition, is referred to as " king of anticancer ".In recent years
Come, food selenium-supply has welcome upsurge, and selenium-rich product has become " favorite " in China food consumption market, and southern exposure health industry is stepped into
" selenium " epoch, but deepening continuously with selenium-rich product development, the safety problems of safety problem, especially Se-rich farm products
It attracts wide attention.Qualified Se-rich farm products should be from the soil rich in selenium element, and crops are by absorption containing in soil
The nutritional ingredients such as selenium, inorganic selenium is converted to Organic Selenium.But the study found that selenium and heavy metal in soil, such as lead (Pb), cadmium
(Cd), there are association relationships for mercury (Hg) and arsenic (As) etc., this be easy to cause the contaminated by heavy metals danger of Se-rich farm products.Its
In, cadmium element is the pollution element of most generally existing.Therefore, it is qualified for exploitation to detect the content of selenium and cadmium element in soil
Se-rich farm products are of great significance.
Currently, it is mainly atomic fluorescence method to measure the method for selenium in soil, but due in soil Se content it is relatively low, and copper,
The high-contents element such as bismuth, nickel, arsenic will produce serious spectra1 interfer-, need to carry out certain pre-treatment, such as in hydrochloric acid medium
Molysite is added to shield the interference etc. of other metal ions in heating reduction hexavalent selenium.The method that cadmium is measured in soil is mainly original
Also there is spectra1 interfer- in sub- absorption process, need that matrix modifier, and this method range of linearity is added when measuring cadmium element
It is very small, it could Accurate Determining after need to further being diluted to enriched sample.Therefore, traditional detection method pre-treatment operation compared with
To be cumbersome, and cannot selenium and cadmium in determination sample simultaneously, seriously reduce detection efficiency.
Inductively coupled plasma-mass spectrometry (ICP-MS) is a kind of quickly and effectively analysis method, with high sensitivity,
The feature that detection limit is low, mass spectrum interferes less, dynamic linear response range is wide, the application in environmental analysis are more and more closed
Note.ICP-MS is ionized however, selenium has higher ionization energy (9.75ev) in argon plasma using argon gas as carrier gas
Degree is relatively low, therefore there is a problem of that sensitivity is poor with ICP-MS detections selenium element.In addition, when ICP-MS measures selenium and cadmium
Mass spectrum interference can be also generated because of argon base ion, isobary and multi-atomic ion etc., seriously affected the accuracy of its result, led
It causes its detection limit to be deteriorated, or even can not directly be measured with ICP-MS.
Invention content
Therefore, the technical problem to be solved in the present invention is to overcome cannot measure selenium and cadmium simultaneously in the prior art, and
ICP-MS has that accuracy and sensitivity is not high in selenium in measuring soil and cadmium element, to provide a kind of accuracy
Good, high sensitivity and the method that selenium and cadmium in soil can be measured simultaneously.
In order to solve the above technical problem, the present invention provides method that is a kind of while measuring selenium and cadmium element in soil,
Include the following steps:
(1) resolution processing is carried out to sample to be tested;
(2) solution after Dynamic Reaction Cell-inductively coupled plasma mass spectrometry detection resolution is used;
Wherein, the relevant parameter of the Dynamic Reaction Cell-inductively coupled plasma mass spectrometry is:Carrier gas:Argon gas;Reaction
Gas:Methane, purity are more than 99.999%, and flow velocity is 0.1~1.0mL/min, 0.1 mL/min of stride;RPq values be 0.45~
0.80, stride 0.05.
Further, step (1) resolution includes graphite resolution and micro-wave digestion in advance.
Further, acid used in the pre- resolution is nitric acid and hydrofluoric acid.
Further, pre- clear up is specially:Sample to be tested described in 0.1g is weighed, sequentially adds 5.0mL thereto
The nitric acid and 1.0mL hydrofluoric acid that mass fraction is 65%, heat up 15min to 140 DEG C, keep 30min.
Further, the micro-wave digestion temperature program is:6min to 120 DEG C of heating keeps 3 min;Heat up 3min
To 150 DEG C, 3min is kept;4min to 190 DEG C of heating keeps 30min.
Further, step (1) further includes carrying out that acid cut is caught up with to hold to the solution after the resolution.
Further, step (1) further includes the solution after catching up with acid cut to hold described in separating-purifying.
Further, step (2) further includes examination criteria blank solution and at least 5 before the solution after detecting the resolution
Selenium, the cadmium hybrid standard working solution of kind various concentration, and canonical plotting is drawn according to testing result.
Further, the standard blank solution is the salpeter solution of volume fraction 5%.
Further, a concentration of 0.2 μ μ of g/L~20 g/L of the selenium of the various concentration, cadmium hybrid standard working solution.
Further, detection process is corrected using internal standard, the interior rhodium solution for being designated as 100 μ g/L of concentration.
Further, containing volume fraction it is respectively also 5% methanol and 5% nitric acid in the rhodium solution.
Technical scheme of the present invention has the following advantages that:
1. method that is provided by the invention while measuring selenium and cadmium element in soil handles sample to be tested by resolution, adopts
Selenium in soil and cadmium are measured simultaneously with Dynamic Reaction Cell-inductively coupled plasma mass spectrometry, by optimizing Dynamic Reaction Cell
Reaction gas flow velocity and quadrupole rod low quality intercept voltage, effectively reduce mass spectrum interference, improve the accuracy of detection and sensitive
Degree.
2. method that is provided by the invention while measuring selenium and cadmium element in soil, to increasing before pedotheque micro-wave digestion
The operation cleared up in advance with graphite resolution instrument, graphite resolution instrument resolution can carry out under normal pressure, and homogeneous heating, reaction is mild, keeps away
The security risk acutely brought is reacted when exempting from direct micro-wave digestion, and extends the service life of micro-wave diminishing pot.The present invention adopts
It clears up the mode being combined with micro-wave digestion in advance with graphite and handles sample to be tested, destroy organic matter and the silicate etc. in sample,
Interference of the organic matter to detection signal, improves the Stability and veracity of analysis when reducing measurement.With concentrated nitric acid-hydrofluoric acid
Acid system is mixed, resolution effect is good, and element loss is few, easy to operate, and obtained digestion solution is clarified, is transparent, and perchloric acid is avoided
Deng the use of acid strong, dangerous high reagent, the harm to operating personnel is reduced, and reduces the dosage of acid, is saved
Reagent cost.
3. method that is provided by the invention while measuring selenium and cadmium element in soil carries out the solution after resolution to catch up with acid cut
Hold, reduce acidity in solution, alleviate corrosion of the acidity to instrument internal, improve the protection to instrument, dilute constant volume, reduces
The concentration of other impurity in sample matrices effectively prevents the interference of sample matrices when ICP-MS detections.After catching up with acid cut to hold
Solution carries out separating-purifying to remove the halide ion in pedotheque background, and it is dry to the mass spectrum of element to be measured to reduce halide ion
It disturbs, ensure that precision of analysis.
4. method that is provided by the invention while measuring selenium and cadmium element in soil, by suitably diluting the dense of prepare liquid
Degree, it is online that rhodium internal standard is added to overcome baseline drift, improve the accuracy of analysis method.Methanol and salpeter solution in rhodium internal standard
Addition, improve the rate of ionization of selenium and cadmium element in inductively coupled plasma electricity body, enhance to a certain extent
The response of low concentration, improves detection limit, improves the accuracy and sensitivity of analysis test.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, other drawings may also be obtained based on these drawings.
Fig. 1 is the canonical plotting for the concentration that the present invention measures selenium;
Fig. 2 is the canonical plotting for the concentration that the present invention measures cadmium.
Specific implementation mode
Technical scheme of the present invention will be clearly and completely described below, it is clear that described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
There is the every other embodiment obtained under the premise of making creative work, shall fall within the protection scope of the present invention.In addition, below
Involved technical characteristic as long as they do not conflict with each other can be mutual in described different embodiments of the present invention
In conjunction with.
In following embodiments:
Instrument and equipment:Icp ms (Perkinelmer, DRC-e), microwave dissolver (CEM,
MarsXpress), graphite resolution instrument (CIF, DS43-260), ultrapure water machine (Millipore, Milli-Q);All vessel exist
Soaked overnight in 20% nitric acid, rinses six times with distilled water repeatedly, finally with ultrapure water it is clean after dry;
Reagent:Nitric acid, hydrofluoric acid are top pure grade or more.
Embodiment 1
Method that is a kind of while measuring selenium and cadmium in soil is present embodiments provided, specially:
(1) sample treatment
The soil natural that acquisition comes is dried, the nylon mesh in the apertures 0.15mm is smashed it through, the soil needed for experiment is made
Sample.0.10g pedotheques (by taking soil changes GBW07403 as an example, verifying the accuracy of this method) are weighed in polytetrafluoro
In ethylene counteracting tank, nitric acid and the 1.0mL hydrofluoric acid that 5.0mL mass fractions are 65% is added, covers inner cover, is placed in graphite resolution
It is cleared up in advance in instrument, pre- temperature program of clearing up is:From room temperature 15min to 140 DEG C, and keep 30min.Pre- resolution finishes cooling
Afterwards, micro-wave digestion in microwave dissolver is placed into, micro-wave digestion temperature program is:From room temperature 6min to 120 DEG C, keep
3min;3min to 150 DEG C of heating keeps 3min;It heats up 4 min to 190 DEG C, keeps 30min.After micro-wave digestion finishes cooling,
Lid is opened, micro-wave diminishing pot is moved back to again in graphite resolution instrument and carries out catching up with acid, catch up with the sour program to be:It heats up from room temperature 15min
To 150 DEG C, 60min is kept.Specimen eliminating liquid is washed out into 50mL plastics volumetric flasks and determined with ultra-pure water after catching up with acid
Hold, takes the Specimen eliminating liquid after 8mL constant volumes to cross and wear peace OnGuard II Ag (2.5 cc) solid phase extraction column (before Ag column uses
First use the ultrapure water wash of 10mL), the 3mL Specimen eliminating liquid flowed out at first is discarded, the 5mL Specimen eliminatings flowed out below are regathered
Liquid, solution flow rate are controlled in 1.0mL/min or so, obtain testing sample solution.Do blank test simultaneously.
(2) optimization of ICP-MS running parameters
The mass spectrum tuning liquid for containing the elements such as Mg, In, U, Ce, Ba with 10 μ g/L optimizes ICP-MS running parameters, such as ICP
RF Power, NEB, Lens Voltage, Analog Stage Voltage, Pulse Stage Voltage, make instrument reach
To optimum state, i.e. In intensity is more than 250000cps, CeO+/Ce+<3%, Ba++/Ba+<3%.Finally determining ICP-MS works
It is as parameter:ICP RF Power 1125W, NEB (Ar2) 0.90mL/min, Lens Voltage 6.25V, Analog
Stage Voltage -2300V, Pulse Stage Voltage 1200V.
(3) foundation of DRC analysis conditions
With CH4For reaction gas, optimize DRC job parameter with 10 μ g/L selenium solutions, such as DRC Mode NEB, DRC Mode
CPV,DRC Mode QRO,DRC Mode CRO.Finally determining DRC job parameter is:DRC Mode NEB(CH4)
0.92mL/min, DRC Mode CPV -21V, DRC Mode QRO-6.5V, DRC Mode CRO-1V;Choose Specimen eliminating liquid
For matrix (M), the selenium and cadmium for adding 10 μ g/L add sample (S) for matrix in the digestion solution, pass through and optimize CH4Flow velocity and RPq
Value establishes the optimum analysis condition that DRC measures selenium and cadmium to inhibit the mass spectrum of selenium and cadmium to interfere, according to signal-to-noise ratio (S/M), finally
Determining optimum analysis condition is as shown in table 1 below.
1 Dynamic Reaction Cell of table measures the analysis condition of selenium and cadmium
4) standard working solution is prepared
With volume fraction be 5% salpeter solution step by step the selenium of diluted concentration 1000mg/L and cadmium standard items in 50mL plastics
In volumetric flask, the selenium and cadmium standard working solution of various concentration are obtained, the selenium and cadmium standard working solution of the various concentration are dense
Degree is respectively:0.2 μ g/L, 1 μ g/L, 5 μ g/L, 10 μ g/L and 20 μ g/L;The salpeter solution for being 5% with volume fraction is dilute step by step
The rhodium inner mark solution for releasing concentration 1000mg/L, it is 100 μ g/L to make rhodium inner mark solution concentration, and contains 5% methanol and 5% nitre
Acid, it is spare.
5) standard curve is drawn
Using the salpeter solution that volume fraction is 5% as standard blank solution, standard blank solution is added into ICP-MS
And the standard working solution that step 4) is prepared, while the online rhodium inner mark solution that step 4) is added and prepares, selenium and cadmium mass number point
Not Cai Yong 80 and 114, the DRC-ICP-MS conditions established using step 2) and step 3) are drawn the standard curve of selenium and cadmium, seen
Fig. 1 and Fig. 2.By Fig. 1 and Fig. 2 it is found that selenium and cadmium related coefficient are respectively 0.99981 and 0.99971, illustrate that it is linear good.
6) sample measures
According to step 5) selenium and cadmium standard curve test condition, determination step 1) testing sample solution.
7) interpretation of result
According to the soil sample weight weighed and detect that the concentration of sample solution calculates the content of selenium and cadmium in pedotheque:
W is constituent content to be measured in soil, unit mg/kg;C is elemental mass concentration to be measured in sample solution, unit
For μ g/L;C0Elemental mass concentration to be measured in the blank solution of position, unit are μ g/L;V is solution constant volume, unit mL;m
Quality, unit g are weighed for soil sample.Analysis result is specifically shown in shown in the following table 2.
Table 2 sample (reference material of soil GBW07403) analysis result
The measured value that Selenium In Some Selenium-rich Biological Samples can be calculated from table 2 is 0.099 ± 0.0035mg/kg, relative standard deviation (RSD)
It is 3.5%;Cadmium detrmination value is 0.062 ± 0.0018mg/kg, and RSD 2.8%, selenium and cadmium measured value are in standard value range
Within.
Comparative example 1
This comparative example 1 provides method that is a kind of while measuring selenium and cadmium in soil, the same above-described embodiment of concrete operations
1, the difference is that, ICP-MS measures selenium and cadmium in mode standard (argon gas), and selenium mass number uses 78 and 82 (correction sides
Journey), cadmium mass number uses 111 and 114 (band correction equations),78Se and82Se results are negative value,111Cd and114Cd measured values point
It Wei not 0.045 ± 0.005mg/kg and 0.094 ± 0.006mg/kg.
Comparative example 2
This comparative example 2 provides method that is a kind of while measuring selenium and cadmium in soil, the same above-described embodiment of concrete operations
1, the difference is that, in DRC analyses, CH4The flow velocity of gas is 0.5mL/min, RPq 0.45, the results show that the inspection of selenium
Rising limit is 0.037mg/kg, and selenium measured value is 0.129 ± 0.015 mg/kg, relative standard deviation 11.6%, the detection limit of cadmium
For 0.021mg/kg, cadmium measured value is 0.084 ± 0.0071, relative standard deviation 8.5%.
In conjunction with Fig. 1, Fig. 2, table 2 and above-mentioned comparative example 1 and 2 it is found that the present invention measures the side of selenium and cadmium in soil simultaneously
The method range of linearity is wide, detection limit is low, accuracy and precision are good, meets requirement of experiment.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments, and it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (12)
1. method that is a kind of while measuring selenium and cadmium element in soil, which is characterized in that include the following steps:
(1) resolution processing is carried out to sample to be tested;
(2) solution after Dynamic Reaction Cell-inductively coupled plasma mass spectrometry detection resolution is used;
Wherein, the relevant parameter of the Dynamic Reaction Cell-inductively coupled plasma mass spectrometry is:Carrier gas:Argon gas;Reaction gas:
Methane, purity are more than 99.999%, and flow velocity is 0.1~1.0mL/min, stride 0.1mL/min;RPq values are 0.45~0.80, step
0.05.
2. according to the method described in claim 1, it is characterized in that, step (1) resolution includes graphite resolution and microwave in advance
Resolution.
3. according to the method described in claim 2, it is characterized in that, acid used in the pre- resolution is nitric acid and hydrofluoric acid.
4. according to the method in claim 2 or 3, which is characterized in that it is described it is pre- resolution be specially:It weighs to be measured described in 0.1g
Sample sequentially adds the nitric acid and 1.0mL hydrofluoric acid of 5.0mL mass fractions 65% thereto, heats up 15min to 140 DEG C, keeps
30min。
5. according to claim 2-4 any one of them methods, which is characterized in that the micro-wave digestion temperature program is:Heating
6min to 120 DEG C, keep 3min;3min to 150 DEG C of heating keeps 3min;4min to 190 DEG C of heating keeps 30min.
6. according to claim 1-5 any one of them methods, which is characterized in that step (1) further includes to after the resolution
Solution carries out that acid cut is caught up with to hold.
7. according to the method described in claim 6, it is characterized in that, step (1) further includes after catching up with acid cut to hold described in separating-purifying
Solution.
8. according to claim 1-7 any one of them methods, which is characterized in that step (2) is molten after detecting the resolution
Further include selenium, the cadmium hybrid standard working solution of examination criteria blank solution and at least five kinds of various concentrations before liquid, and according to detection
As a result canonical plotting is drawn.
9. according to the method described in claim 8, it is characterized in that, the standard blank solution is the nitric acid of volume fraction 5%
Solution.
10. method according to claim 8 or claim 9, which is characterized in that the selenium of the various concentration, the work of cadmium hybrid standard
A concentration of 0.2 μ μ of g/L~20 g/L of solution.
11. according to claim 1-10 any one of them methods, which is characterized in that carry out school to detection process using internal standard
Just, the interior rhodium solution for being designated as 100 μ g/L of concentration.
12. according to the method for claim 11, which is characterized in that be also respectively containing volume fraction in the rhodium solution
5% methanol and 5% nitric acid.
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| CN110308197A (en) * | 2019-08-09 | 2019-10-08 | 福建省农业科学院农业质量标准与检测技术研究所 | Inductively coupled plasma mass spectrometry measures the detection method of Theil indices in soil |
| CN112557560A (en) * | 2020-12-23 | 2021-03-26 | 河北省地质实验测试中心 | Detection method for detecting selenate and selenite in soil by HPLC-ICP-MS |
| CN112782174A (en) * | 2020-12-25 | 2021-05-11 | 西南化工研究设计院有限公司 | High-frequency electrodeless argon discharge ionization detector and method for analyzing sulfur and phosphorus compounds in gas |
| CN118067695A (en) * | 2024-04-17 | 2024-05-24 | 四川交通职业技术学院 | Method for measuring cadmium content in organic soil by ICP-MS |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110308197A (en) * | 2019-08-09 | 2019-10-08 | 福建省农业科学院农业质量标准与检测技术研究所 | Inductively coupled plasma mass spectrometry measures the detection method of Theil indices in soil |
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| CN112782174A (en) * | 2020-12-25 | 2021-05-11 | 西南化工研究设计院有限公司 | High-frequency electrodeless argon discharge ionization detector and method for analyzing sulfur and phosphorus compounds in gas |
| CN118067695A (en) * | 2024-04-17 | 2024-05-24 | 四川交通职业技术学院 | Method for measuring cadmium content in organic soil by ICP-MS |
| CN118067695B (en) * | 2024-04-17 | 2024-06-25 | 四川交通职业技术学院 | Method for measuring cadmium content in organic soil by ICP-MS |
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